Potassium Carbonate → HCID 21109918, compound

HRID 1766178Notes

Reaction equation

HRID 1766178 reaction equation
C([NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][CH2:13][C:14]([OH:16])=[O:15])=[CH:7][C:6]=1[Br:17])(=O)C.C(=O)([O-])[O-].[K+].[K+]>Cl>[NH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][CH2:13][C:14]([OH:16])=[O:15])=[CH:7][C:6]=1[Br:17]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 21109916HCID 21109916, compound

Product 1

HCID 21109918HCID 21109918, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A mixture of 0.13 g (0.008662 mol) of 4-acetylamino-3-bromobenzenebutanoic acid and 10 ml of conc. hydrochloric acid was refluxed for 24 hours. The colourless, needle-shaped crystals of Rf 0.53 (eluant: dichloromethane/methanol 9/1 v/v) precipitated after cooling were identified by spectroscopy as the hydrochloride of the desired 4-amino-3-bromobenzenebutanoic acid. The crystals were dissolved in a little water, and the solution formed was adjusted to pH 6 using concentrated potassium carbonate solution. The precipitate was suction filtered, washed with water and dried in a circulating air dryer at 60° C. Yield: 1.35 g (60% of theoretical).

Workup

  1. temperaturewas refluxed for 24 hours
  2. customThe colourless, needle-shaped crystals of Rf 0.53 (eluant: dichloromethane/methanol 9/1 v/v) precipitated
  3. temperatureafter cooling
  4. dissolutionThe crystals were dissolved in a little water
  5. customthe solution formed
  6. filtrationfiltered
  7. washwashed with water
  8. customdried in a circulating air dryer at 60° C

Sources & evidence

ORD record
ord-02cf11f761dc4abf91635bcba18b75a9
Source dataset
uspto-grants-2007_06
Patent number
US07230001B1

Reaction notes

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